CN111203286B - Preparation device and method of catalyst for producing vinyl acetate by acetylene method - Google Patents
Preparation device and method of catalyst for producing vinyl acetate by acetylene method Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title abstract description 94
- 238000002360 preparation method Methods 0.000 title abstract description 42
- 238000000034 method Methods 0.000 title abstract description 35
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 title abstract description 21
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 title abstract description 19
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 title abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 121
- 238000001035 drying Methods 0.000 abstract description 112
- 238000004064 recycling Methods 0.000 abstract description 51
- 239000007787 solid Substances 0.000 abstract description 46
- 238000005470 impregnation Methods 0.000 abstract description 35
- 238000003860 storage Methods 0.000 abstract description 19
- 230000000694 effects Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000011049 filling Methods 0.000 abstract description 4
- 238000004148 unit process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 114
- 239000007789 gas Substances 0.000 description 105
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 28
- 239000007788 liquid Substances 0.000 description 27
- 238000007598 dipping method Methods 0.000 description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 22
- 229910052799 carbon Inorganic materials 0.000 description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 15
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 15
- 239000004246 zinc acetate Substances 0.000 description 15
- 229910052757 nitrogen Inorganic materials 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 13
- 239000000463 material Substances 0.000 description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 12
- 239000002994 raw material Substances 0.000 description 12
- 239000000843 powder Substances 0.000 description 7
- 238000001179 sorption measurement Methods 0.000 description 7
- 229920006395 saturated elastomer Polymers 0.000 description 6
- 239000011787 zinc oxide Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 125000004122 cyclic group Chemical group 0.000 description 4
- 239000005997 Calcium carbide Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 2
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- MGLUJXPJRXTKJM-UHFFFAOYSA-L bismuth subcarbonate Chemical compound O=[Bi]OC(=O)O[Bi]=O MGLUJXPJRXTKJM-UHFFFAOYSA-L 0.000 description 2
- 229940036358 bismuth subcarbonate Drugs 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052740 iodine Inorganic materials 0.000 description 2
- 239000011630 iodine Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 229920002689 polyvinyl acetate Polymers 0.000 description 2
- 239000011118 polyvinyl acetate Substances 0.000 description 2
- 239000008234 soft water Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- CLZWAWBPWVRRGI-UHFFFAOYSA-N tert-butyl 2-[2-[2-[2-[bis[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]amino]-5-bromophenoxy]ethoxy]-4-methyl-n-[2-[(2-methylpropan-2-yl)oxy]-2-oxoethyl]anilino]acetate Chemical compound CC1=CC=C(N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)C(OCCOC=2C(=CC=C(Br)C=2)N(CC(=O)OC(C)(C)C)CC(=O)OC(C)(C)C)=C1 CLZWAWBPWVRRGI-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229920002978 Vinylon Polymers 0.000 description 1
- 239000011354 acetal resin Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 229920006163 vinyl copolymer Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0203—Impregnation the impregnation liquid containing organic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/009—Preparation by separation, e.g. by filtration, decantation, screening
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0205—Impregnation in several steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0207—Pretreatment of the support
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0209—Impregnation involving a reaction between the support and a fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0213—Preparation of the impregnating solution
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0236—Drying, e.g. preparing a suspension, adding a soluble salt and drying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/04—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides onto unsaturated carbon-to-carbon bonds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/30—Addition reactions at carbon centres, i.e. to either C-C or C-X multiple bonds
- B01J2231/32—Addition reactions to C=C or C-C triple bonds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation device and a preparation method of a catalyst for producing vinyl acetate by an acetylene method, wherein an impregnating solution preparation tank, a feed pump, a vacuum pump, a gas-solid separator, a blower, an impregnating drying tower, a catalyst storage tank, a vibrating screen, a filter, a recycling pump, a bag filter, a Roots blower, a heater, a demister and an induced draft fan are arranged, and the catalyst for producing vinyl acetate by the acetylene method is prepared by four unit processes of impregnating solution preparation, activated carbon filling, circulating impregnation and catalyst drying. The catalyst preparation method and the device effectively improve the activity of the catalyst, prolong the service cycle of the catalyst and ensure stable production.
Description
Technical Field
The invention relates to a preparation device and a preparation method of a catalyst for producing vinyl acetate by an acetylene method.
Background
Vinyl Acetate (VAC) is an important chemical raw material, has strong polymerization capability because of containing unsaturated vinyl in the molecular structure, and is widely used for producing a series of chemical and chemical fiber products such as polyvinyl acetate (PVAC), polyvinyl alcohol, paint, slurry, adhesive, vinylon, film, vinyl copolymer resin, acetal resin and the like, and the application thereof relates to various industries.
The synthesis method of vinyl acetate has evolved for decades, and at present, two methods, namely an ethylene gas phase method and an acetylene gas phase method, are mainly the acetylene method of calcium carbide in China. The german scientist Muqaen in 1922 found that vinyl acetate could be successfully synthesized under the catalysis of zinc acetate-activated carbon. Then during the second world war, the german hurst company has industrialized the synthesis of vinyl acetate. After VAC was industrially synthesized by japan colali in 1968 using the vapor phase method of bayer catalyst technology, the ethylene method was rapidly developed. However, the acetylene method has the characteristics of simple technology, low catalyst cost, good activity and the like, and has strong development potential in some countries and regions. In areas with rich calcium carbide resources and natural gas resources, the acetylene gas phase method has stronger competitiveness due to the advantages of sufficient raw materials and energy sources, low cost and the like, so that the development of the high-efficiency catalyst for the acetylene gas phase method has quite important significance.
For a long time, many scholars at home and abroad have studied on improving the activity and service life of a catalyst for producing vinyl acetate by an acetylene method mainly focused on the research fields of changing active components, improving the specific surface area of active carbon, optimizing the pore structure and surface functional groups of the active carbon, optimizing the loading of the active components, optimizing catalyst auxiliaries and the like. The practice proves that the active carbon is irreplaceable as a catalyst carrier for synthesizing the vinyl acetate by an acetylene method. The catalyst used for synthesizing vinyl acetate by the calcium carbide acetylene gas phase method in China is zinc acetate-activated carbon all the time, but the catalyst has the defects of quick activity reduction, low service life and the like, and in the use process, the catalyst is frequently replaced, wastes a large amount of manpower and material resources and seriously affects the production continuity and stability.
Disclosure of Invention
The invention aims to provide a preparation device and a preparation method of a catalyst for producing vinyl acetate by an acetylene method, so that the problem of rapid reduction of the activity of the catalyst can be solved, the service efficiency of the catalyst in the vinyl acetate production process is improved, the replacement period of the catalyst is prolonged, and therefore, manpower and material resources are greatly saved, and high-efficiency and stable production is ensured.
The aim of the invention can be achieved by the following technical scheme:
the invention discloses a preparation device of a catalyst for producing vinyl acetate by an acetylene method, which comprises an impregnating solution preparation tank, a feed pump, a vacuum pump, a gas-solid separator, a blower, an impregnating drying tower, a catalyst storage tank, a vibrating screen, a filter, a recycling pump, a bag filter, a Roots blower, a heater, a demister and an induced draft fan;
a centrifugal pump is arranged at the upper part of the impregnating solution preparing tank and is connected with a stirrer arranged in the impregnating solution preparing tank; the upper part of the impregnating solution preparing tank is provided with a raw material feeding port and an impregnating solution recycling inlet of the impregnating solution preparing tank, and the lower part of the impregnating solution preparing tank is provided with an impregnating solution outlet of the impregnating solution preparing tank; a steam heating coil is arranged at the periphery of the impregnating solution preparing tank, and a steam inlet of the impregnating solution preparing tank and a steam condensate outlet of the impregnating solution preparing tank are arranged on the steam heating coil; a feed pump inlet and a feed pump outlet are arranged on the feed pump; a vacuum pump inlet and a vacuum pump outlet are arranged on the vacuum pump; a filter is arranged in the gas-solid separator, the lower part is provided with a gas-solid separator active carbon inlet and a gas-solid separator active carbon outlet, and the upper part is provided with a gas outlet of the gas-solid separator and a compressed gas inlet of the gas-solid separator; a blower inlet and a blower outlet are arranged on the blower; the lower part of the impregnating drying tower is provided with an impregnating drying tower impregnating liquid inlet, an impregnating drying tower active carbon inlet and an impregnating drying tower catalyst outlet, the upper part is provided with an impregnating drying tower gas outlet and an impregnating drying tower overflow liquid outlet, the middle upper part is provided with an impregnating drying tower hot water inlet and an impregnating drying tower hot nitrogen outlet, and the middle lower part is provided with an impregnating drying tower hot water outlet, an impregnating drying tower recycling impregnating liquid outlet, an impregnating drying tower hot nitrogen inlet and an impregnating drying tower circulating gas inlet; a catalyst inlet of the catalyst storage tank and a catalyst outlet of the catalyst storage tank are arranged in the middle of the catalyst storage tank; a vibrating screen catalyst inlet and a vibrating screen catalyst outlet are arranged at the upper part of the vibrating screen; the middle part of the filter is provided with a filter overflow liquid inlet and a filter recycling impregnating liquid outlet, and the lower part of the filter is provided with a filter recycling impregnating liquid inlet; a recycling pump inlet and a recycling pump outlet are arranged on the recycling pump; the upper part of the bag filter is provided with a bag filter gas inlet and a bag filter gas outlet, and the bottom is provided with a bag filter powder outlet; the Roots blower is provided with a Roots blower inlet and a Roots blower outlet; the upper part of the heater is provided with a first heater gas inlet, a second heater gas inlet and a heater steam inlet, and the lower part of the heater is provided with a heater steam condensate outlet and a heater circulating gas outlet; the upper part of the demister is provided with a demister gas inlet, and the lower part of the demister is provided with a demister gas outlet; an induced draft fan inlet and an induced draft fan outlet are arranged on the induced draft fan;
the impregnating solution outlet of the impregnating solution preparation tank is connected with the inlet of the charging pump; the outlet of the feed pump is connected with the impregnating solution inlet of the impregnating drying tower; the outlet of the vacuum pump is connected with the active carbon inlet of the gas-solid separator; the gas-solid separator active carbon outlet is connected with the inlet of the blower; the outlet of the air blower is connected with the active carbon inlet of the impregnation drying tower; the catalyst outlet of the impregnation drying tower is connected with the catalyst inlet of the catalyst storage tank; the catalyst outlet of the catalyst storage tank is connected with the catalyst inlet of the vibrating screen; the gas outlet of the impregnation drying tower is connected with the gas inlet of the bag filter; the bag filter gas outlet is respectively connected with the Roots blower inlet and the demister gas inlet; the Roots blower outlet is connected with the heater gas first inlet; the demister gas outlet is connected with the inlet of the induced draft fan; the outlet of the induced draft fan is connected with the second gas inlet of the heater; the heater circulating gas outlet is connected with the impregnating drying tower circulating gas inlet; the overflow liquid outlet of the impregnation drying tower is connected with the overflow liquid inlet of the filter; the recycling impregnating solution outlet of the impregnating drying tower is connected with the recycling pump inlet; the outlet of the recycling pump is connected with the inlet of the filter recycling impregnating solution; the filter recycling impregnating solution outlet is connected with the impregnating solution inlet of the impregnating solution preparation tank recycling impregnating solution.
The invention also discloses a preparation method of the catalyst for producing vinyl acetate by using the acetylene method, which is carried out by using the device and comprises four unit processes of impregnating solution preparation, activated carbon filling, circulating impregnation and catalyst drying. The method comprises the following specific steps:
(1) Preparation of impregnating solution
Adding raw materials required by preparing the impregnating solution from a raw material feed port of an impregnating solution preparation tank, wherein the raw materials comprise acetic acid, zinc oxide, bismuth subcarbonate and desalted soft water; introducing low-pressure saturated steam into a steam heating coil pipe at the periphery of an impregnating solution preparation tank from a steam inlet of the impregnating solution preparation tank, performing non-contact heat exchange with materials in the tank, heating the materials in the heating tank to a certain temperature, and delivering steam condensate generated after heat exchange from a steam condensate outlet of the impregnating solution preparation tank; simultaneously starting a centrifugal pump and a stirrer of the impregnating solution preparation tank to enable materials in the tank to flow, uniformly mixing, fully reacting acetic acid with zinc oxide to generate zinc acetate aqueous solution, and completing the reaction to obtain the impregnating solution;
(2) Activated carbon packing
Firstly, sucking purchased activated carbon into a gas-solid separator through a vacuum pump from an activated carbon inlet of the gas-solid separator; a filter is arranged in the gas-solid separator, and the gas generated after the filtration is discharged into the atmosphere through a gas outlet of the gas-solid separator; after the amount of activated carbon added from the activated carbon inlet of the gas-solid separator reaches a certain amount, closing the vacuum pump, and introducing compressed air into the gas-solid separator from the compressed gas inlet of the gas-solid separator to ensure that the gas-solid separator is positive in pressure so as to facilitate the activated carbon to fall off from the bottom of the gas-solid separator under the blocking action of the filter; under the action of a blower, the activated carbon filled at the bottom of the gas-solid separator is sent to the impregnation drying tower from the activated carbon inlet of the impregnation drying tower through the activated carbon outlet of the gas-solid separator for filling;
repeating the above charging operation steps until the activated carbon fed from the activated carbon inlet of the impregnation drying tower reaches the charging amount;
(3) Cyclic impregnation
The prepared impregnating solution is circularly sent into an impregnating drying tower from an impregnating solution inlet of the impregnating drying tower through a feeding pump from an impregnating solution outlet of an impregnating solution preparation tank, and the activated carbon filled in the step (2) is impregnated;
in the dipping process, hot water is added into the dipping drying tower through a hot water inlet of the dipping drying tower, and non-contact heat exchange is carried out between the hot water and materials in the tower, so that the stability of the dipping temperature is ensured; hot water after heat exchange is discharged from a hot water outlet of the impregnation drying tower; simultaneously, a certain liquid level is maintained in the impregnating and drying tower all the time, so that the activated carbon is immersed, redundant impregnating solution flows out of the tower from an overflow solution outlet of the impregnating and drying tower, a filter is added into an overflow solution inlet of the filter connected with the overflow solution outlet of the impregnating and drying tower to filter and remove active carbon residues, and then the impregnating solution is recycled from an impregnating solution inlet of an impregnating solution preparation tank to the impregnating solution preparation tank through a recycling impregnating solution outlet of the filter;
meanwhile, monitoring the concentration of zinc acetate at the overflow liquid outlet of the impregnation drying tower, and when the concentration of zinc acetate is not changed any more, the adsorption of the activated carbon to the impregnation liquid is saturated, namely, the cyclic impregnation process of the activated carbon is completed, and the catalyst is obtained;
(4) Drying of the catalyst
Closing a feeding pump, stopping adding impregnating liquid into the impregnating drying tower, and starting a recycling pump; delivering the impregnating solution in the impregnating drying tower from an impregnating solution recycling outlet of the impregnating drying tower, delivering the impregnating solution to a filter for filtering through a recycling pump from a filter recycling impregnating solution inlet, and adding the filtered recycling impregnating solution into an impregnating solution preparation tank for recycling through the impregnating solution recycling inlet of the impregnating solution preparation tank from the filter recycling impregnating solution outlet;
the catalyst obtained in the step (3) is naturally dripped in an impregnating and drying tower, and then the catalyst is indirectly heated under the action of hot water pipes distributed in the impregnating and drying tower after the natural dripping and drying are finished; simultaneously, hot nitrogen is introduced into the impregnating drying tower through a hot nitrogen inlet of the impregnating drying tower, and the catalyst is directly heated and dried;
the dried gas carries a small amount of activated carbon powder, is discharged into a bag filter through a gas inlet of the bag filter from a gas outlet of the impregnation drying tower, and is dedusted through the bag filter; the gas after dust removal is sent out from a gas outlet of the bag filter, and the obtained powder is discharged from a powder outlet of the bag filter;
pressurizing part of gas sent out from a gas outlet of the bag filter by a Roots blower, and adding the gas into the heater from a first gas inlet of the heater; the residual gas sent out by the gas outlet of the bag filter enters the demister from the gas inlet of the demister to be cooled and demisted, and after the treatment, the residual gas is pressurized by the gas outlet of the demister through a draught fan and then is added into the heater from the second gas inlet of the heater;
introducing steam into the heater through a steam inlet of the heater, and performing non-contact heat exchange with gas in the heater; the steam condensate after heat exchange is discharged from a steam condensate outlet of a heater, and the gas after temperature rise is sent out from a circulating gas outlet of the heater and then is added into the impregnating drying tower for recycling through a circulating gas inlet of the impregnating drying tower;
and after the catalyst in the impregnation drying tower is dried, adding the catalyst into a catalyst storage tank through a catalyst inlet of the catalyst storage tank, and packaging through a vibrating screen to obtain a catalyst finished product.
Further, in the step (1), the temperature of the materials in the impregnating solution preparing tank to be heated is 60-80 ℃.
Further, in the step (1), the reaction equation of acetic acid and zinc oxide is ZnO+2HAC→Zn (AC) 2 +H 2 O。
Further, in the step (2), the purchased activated carbon is 28-40 meshes, the iodine adsorption value is more than or equal to 1000mg/g, the strength is more than or equal to 95%, and the water content is less than or equal to 3%.
Further: in the step (3), the impregnation temperature of the impregnation drying tower is 80-90 ℃; when adsorption is saturated, the concentration of zinc acetate at the overflow liquid outlet (6 e) of the impregnation drying tower is 18-21%, and the adsorption quantity of the activated carbon to the zinc acetate is 31-35g of zinc acetate/100 g of activated carbon.
Further, in the step (4), the temperature of the hot nitrogen (G) is 80-90 ℃, and the moisture content of the catalyst after the drying is not higher than 0.5%.
Further, in the step (4), the volume ratio of the gas fed into the Roots blower to the gas fed into the demister is 7:3.
Compared with the prior art, the invention has the beneficial effects that:
according to the device and the method, the active carbon is excessively impregnated in the impregnating and drying tower, and the indirect heating of the hot water pipe in the tower and the direct heating of the hot nitrogen are combined, so that zinc acetate is uniformly distributed on the surface and the inside of the active carbon, the activity of the catalyst is effectively improved, the service cycle of the catalyst is effectively prolonged, the workload when the catalyst is replaced and the consumption of materials are reduced, and the device and the method have good economic benefits.
Drawings
FIG. 1 is a schematic diagram of a catalyst preparation apparatus for producing vinyl acetate by acetylene method according to the present invention, wherein reference numerals are used in the drawings:
1 is an impregnating solution preparation tank, 2 is a feed pump, 3 is a vacuum pump, 4 is a gas-solid separator, 5 is a blower, 6 is an impregnating drying tower, 7 is a catalyst storage tank, 8 is a vibrating screen, 9 is a filter, 10 is a recycling pump, 11 is a bag filter, 12 is a Roots blower, 13 is a heater, 14 is a demister, and 15 is an induced draft fan;
1-1 is a centrifugal pump, 1-2 is a stirrer, 1a is a raw material feed port, 1b is an impregnating solution outlet of an impregnating solution preparation tank, 1c is an impregnating solution recycling inlet of the impregnating solution preparation tank, 1d is an impregnating solution preparation tank steam inlet, and 1e is an impregnating solution preparation tank steam condensate outlet; 2a is a feed pump inlet, 2b is a feed pump outlet; 3a is the vacuum pump inlet, 3b is the vacuum pump outlet; 4-1 is a filter, 4a is a gas-solid separator activated carbon inlet, 4b is a gas-solid separator activated carbon outlet, 4c is a gas-solid separator gas outlet, and 4d is a gas-solid separator compressed gas inlet; 5a is the blower inlet and 5b is the blower outlet; 6a is an impregnating solution inlet of an impregnating drying tower, 6b is an active carbon inlet of the impregnating drying tower, 6c is a catalyst outlet of the impregnating drying tower, 6d is a gas outlet of the impregnating drying tower, 6e is an overflow liquid outlet of the impregnating drying tower, 6f is a hot water inlet of the impregnating drying tower, 6g is a hot water outlet of the impregnating drying tower, 6h is a recycling impregnating solution outlet of the impregnating drying tower, 6i is a hot nitrogen outlet of the impregnating drying tower, 6j is a hot nitrogen inlet of the impregnating drying tower, and 6k is a circulating gas inlet of the impregnating drying tower; 7a is a catalyst inlet of the catalyst storage tank, and 7b is a catalyst outlet of the catalyst storage tank; 8a is a vibrating screen catalyst inlet, 8b is a vibrating screen catalyst outlet; 9a is a filter overflow liquid inlet, 9b is a filter recycling impregnating liquid outlet, and 9c is a filter recycling impregnating liquid inlet; 10a is the recycling pump inlet, and 10b is the recycling pump outlet; 11a is a bag filter gas inlet, 11b is a bag filter gas outlet, and 11c is a bag filter powder outlet; 12a is the Roots blower inlet, 12b is the Roots blower outlet; 13a is a heater first gas inlet, 13b is a heater second gas inlet, 13c is a heater recycle gas outlet, 13d is a heater steam inlet 13d,13e is a heater steam condensate outlet; 14a is a demister gas inlet and 14b is a demister gas outlet; 15a is the inlet of the induced draft fan, 15b is the outlet of the induced draft fan;
a represents the raw materials required for preparing the impregnating solution, B represents low-pressure saturated steam, C represents steam condensate, D represents activated carbon, E represents gas, F represents hot water, G represents hot nitrogen, H represents catalyst finished product, I represents powder, and Q represents compressed air.
Detailed Description
The following describes embodiments of the present invention in detail with reference to the accompanying drawings, and the embodiments and specific operation procedures are given by the embodiments of the present invention under the premise of the technical solution of the present invention, but the scope of protection of the present invention is not limited to the following embodiments.
As shown in fig. 1, the present embodiment first provides a preparation apparatus for a catalyst for producing vinyl acetate by an acetylene method, comprising a impregnating solution preparing tank 1, a feed pump 2, a vacuum pump 3, a gas-solid separator 4, a blower 5, an impregnating drying tower 6, a catalyst storage tank 7, a vibrating screen 8, a filter 9, a recycling pump 10, a bag filter 11, a roots blower 12, a heater 13, a demister 14 and an induced draft fan 15.
The upper part of the impregnating solution preparing tank 1 is provided with a centrifugal pump 1-1, and the centrifugal pump 1-1 is connected with a stirrer 1-2 arranged in the impregnating solution preparing tank; the upper part of the impregnating solution preparing tank 1 is provided with a raw material feed port 1a and an impregnating solution recycling inlet 1c of the impregnating solution preparing tank, and the lower part is provided with an impregnating solution outlet 1b of the impregnating solution preparing tank; a steam heating coil is arranged at the periphery of the impregnating solution preparing tank, and a steam inlet 1d of the impregnating solution preparing tank and a steam condensate outlet 1e of the impregnating solution preparing tank are arranged on the steam heating coil; a feed pump inlet 2a and a feed pump outlet 2b are arranged on the feed pump 2; a vacuum pump inlet 3a and a vacuum pump outlet 3b are arranged on the vacuum (3; a filter 4-1 is arranged in the gas-solid separator 4; a gas-solid separator active carbon inlet 4a and a gas-solid separator active carbon outlet 4b are arranged on the lower part, a gas-solid separator gas outlet 4c and a gas-solid separator compressed gas inlet 4d are arranged on the upper part; a blower inlet 5a and a blower outlet 5b are arranged on the blower 5; a dipping drying tower dipping liquid inlet 6a, a dipping drying tower active carbon inlet 6b and a dipping drying tower catalyst outlet 6c are arranged on the lower part, a dipping drying tower gas outlet 6d and a dipping drying tower overflow liquid outlet 6e are arranged on the upper part, a dipping drying tower hot water inlet 6f and a dipping drying tower hot nitrogen outlet 6i are arranged on the upper part, a dipping drying tower hot water outlet 6g, a dipping drying tower recycling dipping liquid outlet 6h, a dipping drying tower hot nitrogen inlet 6j and a dipping drying tower circulating gas inlet 6k are arranged on the lower part, a catalyst storage tank 7a and a catalyst storage tank 7b are arranged on the middle part, a dipping drying tower dipping liquid inlet 6b and a filter inlet 13a filter inlet 11a and a filter inlet 13b are arranged on the lower part, a filter inlet 11b is arranged on the upper part, a filter inlet 13a filter inlet 11b is arranged on the lower part, a filter inlet 11b is arranged on the vacuum pump inlet 13b, a filter inlet 12b is arranged on the lower part, a filter inlet 11b is arranged on the bottom part, the lower part is provided with a heater steam condensate outlet 13e and a heater circulating gas outlet 13c; a demister gas inlet 14a is arranged at the upper part of the demister 14, and a demister gas outlet 14b is arranged at the lower part of the demister 14; the induced draft fan 15 is provided with an induced draft fan inlet 15a and an induced draft fan outlet 15b.
The impregnating solution outlet 1b of the impregnating solution preparation tank is connected with the inlet 2a of the charging pump; the outlet 2b of the feed pump is connected with the impregnating solution inlet 6a of the impregnating drying tower; the vacuum pump outlet 3b is connected with the gas-solid separator active carbon inlet 4 a; the gas-solid separator activated carbon outlet 4b is connected with the blower inlet 5 a; the blower outlet 5b is connected with the activated carbon inlet 6b of the impregnation drying tower; the catalyst outlet 6c of the impregnation drying tower is connected with the catalyst inlet 7a of the catalyst storage tank; the catalyst outlet 7b of the catalyst storage tank is connected with the catalyst inlet 8a of the vibrating screen; the gas outlet 6d of the impregnation drying tower is connected with the gas inlet 11a of the bag filter; the bag filter gas outlet 11b is connected with the Roots blower inlet 12a and the demister gas inlet 14a respectively; the Roots blower outlet 12b is connected with the heater gas first inlet 13 a; the demister gas outlet 14b is connected with an induced draft fan inlet 15 a; the induced draft fan outlet 15b is connected with the heater second gas inlet 13 b; the heater recycle gas outlet 13c is connected with the impregnation drying tower recycle gas inlet 6k; the overflow liquid outlet 6e of the impregnation drying tower is connected with the overflow liquid inlet 9a of the filter; the recycled impregnating solution outlet 6h of the impregnating drying tower is connected with the recycling pump inlet 10 a; the recycling pump outlet 10b is connected with the filter recycling impregnating solution inlet 9c; the filter recycling impregnating solution outlet 9b is connected with the impregnating solution inlet 1c of the impregnating solution preparing tank recycling impregnating solution.
In the specific implementation, the gas-solid separator 4 is used for removing the entrained gas from the fed activated carbon, and a certain vacuum degree is kept in the tower in the filling process, so that the activated carbon is conveniently sucked, and the filter in the tower plays an important role in separating the activated carbon from the gas. After the activated carbon is sucked into a certain amount, the vacuum pump is closed, compressed air is introduced through a compressed air inlet arranged at the upper part, so that the inside of the gas-solid separator is ensured to keep positive pressure, and the activated carbon blanking is facilitated.
In specific implementation, the heater 13 is of a tube type structure, and gases and vapors with different temperatures are introduced outside the tube to exchange heat, so that the effect of heating circulating gas is achieved.
In particular embodiments, the mist eliminator 14 is a plate structure, with the purpose of removing droplets that may be present in the dried gas, and reducing corrosion of subsequent heaters.
The preparation method of the catalyst for producing vinyl acetate by using the acetylene method is carried out by using the device and comprises the following steps:
(1) Preparation of impregnating solution
Raw material A required by preparing the impregnating solution is added into a raw material feed port 1a of the impregnating solution preparation tank, and the raw materials comprise acetic acid, zinc oxide, bismuth subcarbonate and desalted soft water, wherein the mass ratio of the raw materials is 220:150:0.6:2000; introducing low-pressure saturated steam B into a steam heating coil pipe at the periphery of the impregnating solution preparing tank through a steam inlet 1d of the impregnating solution preparing tank, performing non-contact heat exchange with materials in the tank, heating the materials in the heating tank to 60-80 ℃, and delivering steam condensate C generated after heat exchange through a steam condensate outlet 1e of the impregnating solution preparing tank; simultaneously, a centrifugal pump 1-1 and a stirrer 1-2 of the impregnating solution preparing tank are started to enable materials in the tank to flow, the materials are uniformly mixed, acetic acid and zinc oxide fully react to generate zinc acetate aqueous solution, and the impregnating solution is obtained after the reaction is completed.
(2) Activated carbon packing
Firstly, sucking purchased activated carbon D into a gas-solid separator through a vacuum pump 3 through a gas-solid separator activated carbon inlet 4 a; the gas-solid separator 4 is internally provided with a filter 4-1, and the gas E generated after the filtration is discharged into the atmosphere through a gas outlet 4c of the gas-solid separator; after the activated carbon added from the activated carbon inlet 4a of the gas-solid separator reaches a certain amount, the vacuum pump 3 is closed, compressed air Q is introduced into the gas-solid separator from the compressed gas inlet 4d of the gas-solid separator, so that the gas-solid separator is positive in pressure, and the activated carbon is convenient to fall off from the bottom of the gas-solid separator under the blocking action of the filter 4-1; activated carbon filled at the bottom of the gas-solid separator is sent to the impregnation drying tower from the activated carbon inlet 6b of the impregnation drying tower for filling through the activated carbon outlet 4b of the gas-solid separator under the action of the blower 5;
repeating the above charging operation steps until the activated carbon charged from the activated carbon inlet 6b of the impregnation drying tower reaches the charging amount;
wherein, the purchased activated carbon is 28-40 meshes, the iodine adsorption value is not less than 1000mg/g, the strength is not less than 95%, and the moisture is not more than 3%.
(3) Cyclic impregnation
The impregnating solution prepared in the step (1) is circularly fed into the impregnating drying tower 6 from an impregnating solution outlet 1b of an impregnating solution preparation tank through an impregnating solution inlet 6a of the impregnating drying tower by a feed pump 2, and the activated carbon D filled in the step (2) is impregnated;
in the dipping process, hot water F is added into the dipping drying tower through a hot water inlet 6F of the dipping drying tower, and non-contact heat exchange is carried out between the hot water F and materials in the tower, so that the stability of the dipping temperature is ensured; hot water after heat exchange is discharged from a hot water outlet 6g of the impregnation drying tower; simultaneously, a certain liquid level is maintained in the impregnating and drying tower all the time, so that the activated carbon is immersed, redundant impregnating solution flows out of the tower from an impregnating and drying tower overflow solution outlet 6e, is added into a filter 9 through a filter overflow solution inlet 9a connected with the impregnating and drying tower overflow solution outlet 6e to remove active carbon residues by filtration, and is recycled through a filter recycling impregnating solution outlet 9b from an impregnating solution recycling impregnating solution inlet 1c to an impregnating solution preparation tank;
meanwhile, monitoring the concentration of zinc acetate at the overflow liquid outlet 6e of the impregnation drying tower, and when the concentration of zinc acetate is not changed any more, saturating the impregnation liquid by the activated carbon to finish the cyclic impregnation process of the activated carbon to obtain a catalyst;
wherein: the dipping temperature of the dipping drying tower is 80-90 ℃; when the adsorption is saturated, the concentration of zinc acetate at the overflow liquid outlet 6e of the impregnation drying tower is 18-20%, and the adsorption quantity of the activated carbon to the zinc acetate is 31-35g zinc acetate/100 g activated carbon.
(4) Drying of the catalyst
Closing the feeding pump 2, stopping feeding the impregnating solution into the impregnating drying tower 6, and starting the recycling pump 10; delivering the impregnating solution in the impregnating drying tower from an impregnating solution recycling outlet 6h of the impregnating drying tower, delivering the impregnating solution to a filter for filtering through a recycling pump 10 from a filter recycling impregnating solution inlet (9 c), and adding the filtered recycling impregnating solution into an impregnating solution preparation tank for recycling through an impregnating solution recycling impregnating solution outlet 9b from the filter recycling impregnating solution inlet 1c;
the catalyst obtained in the step 3 is naturally dripped in an impregnating and drying tower, and the catalyst is indirectly heated under the action of hot water pipes distributed in the impregnating and drying tower after the natural dripping and drying are finished; simultaneously, hot nitrogen G is introduced into the impregnating drying tower through a hot nitrogen inlet 6j of the impregnating drying tower, and the catalyst is directly heated and dried;
the dried gas carries a small amount of activated carbon powder and is discharged into a bag filter through a gas inlet 11a of the bag filter by a gas outlet 6d of the impregnation drying tower, and dust is removed through the bag filter; the dedusted gas is sent out from a bag filter gas outlet 11b, and the obtained powder I is discharged from a bag filter powder outlet 11c;
part of the gas sent out from the bag filter gas outlet 11b is pressurized by the Roots blower 12 and is added into the heater 13 from the heater first gas inlet 13 a; the rest gas sent out by the bag filter gas outlet 11b enters the demister through the demister gas inlet 14a to be cooled and demisted, and after treatment, the gas is pressurized by the demister gas outlet 14b through the induced draft fan 15 and then is added into the heater through the heater second gas inlet 13 b;
introducing steam B into the heater through a heater steam inlet 13d, and performing non-contact heat exchange with gas in the heater; the steam condensate C after heat exchange is discharged from a heater steam condensate outlet 13e, and the gas after temperature rise is sent out from a heater circulating gas outlet 13C and then is added into the impregnating drying tower for recycling through a circulating gas inlet 6k of the impregnating drying tower;
after the catalyst in the impregnation drying tower is dried, adding the catalyst into the catalyst storage tank 7 through a catalyst inlet 7a of the catalyst storage tank, and packaging the catalyst through a vibrating screen 8 to obtain a catalyst finished product H;
wherein: the temperature of the introduced hot nitrogen (G) is 80-90 ℃, and the moisture content of the catalyst after drying is not higher than 0.5%; the volume ratio of the gas fed to the Roots blower to the gas fed to the mist eliminator was 7:3.
The catalyst prepared by the method of the embodiment has the advantages that the active components are uniformly distributed in the carrier active carbon, the problems of short service life, frequent replacement times and labor waste of the original catalyst are solved, the replacement period is effectively prolonged, the public engineering resources such as steam, circulating water and the like are reduced to a great extent, the production stability is facilitated, and the catalyst has good economic benefits.
The above description is illustrative of the invention and is not intended to be limiting, but is to be construed as being included within the spirit and scope of the invention.
Claims (5)
1. A preparation device of a catalyst for producing vinyl acetate by an acetylene method is characterized in that: the device comprises a impregnating solution preparation tank (1), a feed pump (2), a vacuum pump (3), a gas-solid separator (4), a blower (5), an impregnating drying tower (6), a catalyst storage tank (7), a vibrating screen (8), a filter (9), a recycling pump (10), a bag filter (11), a Roots blower (12), a heater (13), a demister (14) and an induced draft fan (15);
a centrifugal pump (1-1) is arranged at the upper part of the impregnating solution preparing tank (1), and the centrifugal pump (1-1) is connected with a stirrer (1-2) arranged in the impregnating solution preparing tank; the upper part of the impregnating solution preparation tank (1) is provided with a raw material feed port (1 a) and an impregnating solution recycling inlet (1 c) of the impregnating solution preparation tank, and the lower part of the impregnating solution preparation tank is provided with an impregnating solution outlet (1 b); a steam heating coil is arranged at the periphery of the impregnating solution preparing tank, and a steam inlet (1 d) of the impregnating solution preparing tank and a steam condensate outlet (1 e) of the impregnating solution preparing tank are arranged on the steam heating coil; a feed pump inlet (2 a) and a feed pump outlet (2 b) are arranged on the feed pump (2); a vacuum pump inlet (3 a) and a vacuum pump outlet (3 b) are arranged on the vacuum pump (3); a filter (4-1) is arranged in the gas-solid separator (4), a gas-solid separator active carbon inlet (4 a) and a gas-solid separator active carbon outlet (4 b) are arranged at the lower part, and a gas outlet (4 c) and a gas inlet (4 d) of the gas-solid separator are arranged at the upper part; a blower inlet (5 a) and a blower outlet (5 b) are arranged on the blower (5); the lower part of the impregnating drying tower (6) is provided with an impregnating drying tower impregnating liquid inlet (6 a), an impregnating drying tower active carbon inlet (6 b) and an impregnating drying tower catalyst outlet (6 c), the upper part is provided with an impregnating drying tower gas outlet (6 d) and an impregnating drying tower overflow liquid outlet (6 e), the middle upper part is provided with an impregnating drying tower hot water inlet (6 f) and an impregnating drying tower hot nitrogen outlet (6 i), and the middle lower part is provided with an impregnating drying tower hot water outlet (6 g), an impregnating drying tower recycling impregnating liquid outlet (6 h), an impregnating drying tower hot nitrogen inlet (6 j) and an impregnating drying tower circulating gas inlet (6 k); a catalyst inlet (7 a) of the catalyst storage tank and a catalyst outlet (7 b) of the catalyst storage tank are arranged in the middle of the catalyst storage tank (7); a vibrating screen catalyst inlet (8 a) and a vibrating screen catalyst outlet (8 b) are arranged at the upper part of the vibrating screen (8); a filter overflow liquid inlet (9 a) and a filter recycling impregnating liquid outlet (9 b) are arranged in the middle of the filter (9), and a filter recycling impregnating liquid inlet (9 c) is arranged at the lower part of the filter; a recycling pump inlet (10 a) and a recycling pump outlet (10 b) are arranged on the recycling pump (10); the upper part of the bag filter (11) is provided with a bag filter gas inlet (11 a) and a bag filter gas outlet (11 b), and the bottom is provided with a bag filter powder outlet (11 c); a Roots blower inlet (12 a) and a Roots blower outlet (12 b) are arranged on the Roots blower (12); the upper part of the heater (13) is provided with a heater first gas inlet (13 a), a heater second gas inlet (13 b) and a heater steam inlet (13 d), and the lower part is provided with a heater steam condensate outlet (13 e) and a heater circulating gas outlet (13 c); a demister gas inlet (14 a) is formed in the upper part of the demister (14), and a demister gas outlet (14 b) is formed in the lower part of the demister; an induced draft fan inlet (15 a) and an induced draft fan outlet (15 b) are arranged on the induced draft fan (15);
the impregnating solution outlet (1 b) of the impregnating solution preparation tank is connected with the inlet (2 a) of the feeding pump; the outlet (2 b) of the feeding pump is connected with the impregnating liquid inlet (6 a) of the impregnating drying tower; the vacuum pump outlet (3 b) is connected with the gas-solid separator activated carbon inlet (4 a); the gas-solid separator activated carbon outlet (4 b) is connected with the blower inlet (5 a); the blower outlet (5 b) is connected with the impregnation drying tower active carbon inlet (6 b); the catalyst outlet (6 c) of the impregnation drying tower is connected with the catalyst inlet (7 a) of the catalyst storage tank; the catalyst outlet (7 b) of the catalyst storage tank is connected with the catalyst inlet (8 a) of the vibrating screen; the dip drying tower gas outlet (6 d) is connected with the bag filter gas inlet (11 a); the bag filter gas outlet (11 b) is respectively connected with the Roots blower inlet (12 a) and the demister gas inlet (14 a); the Roots blower outlet (12 b) is connected with the heater gas first inlet (13 a); the demister gas outlet (14 b) is connected with the induced draft fan inlet (15 a); the induced draft fan outlet (15 b) is connected with the heater second gas inlet (13 b); the heater circulating gas outlet (13 c) is connected with the impregnating drying tower circulating gas inlet (6 k); the overflow liquid outlet (6 e) of the impregnation drying tower is connected with the overflow liquid inlet (9 a) of the filter; the recycled impregnating solution outlet (6 h) of the impregnating drying tower is connected with the recycling pump inlet (10 a); the recycling pump outlet (10 b) is connected with the filter recycling impregnating solution inlet (9 c); the filter recycling impregnating solution outlet (9 b) is connected with the impregnating solution recycling inlet (1 c) of the impregnating solution preparation tank.
2. A preparation method of a catalyst for producing vinyl acetate by an acetylene method is characterized by comprising the following steps: the device of claim 1, comprising four unit processes of impregnating solution preparation, activated carbon filling, circulating impregnation and catalyst drying, wherein the method comprises the following specific steps:
(1) Preparation of impregnating solution
Adding raw materials (A) required by preparing the impregnating solution through a raw material feed port (1 a) of an impregnating solution preparation tank, wherein the raw materials comprise acetic acid, zinc oxide, bismuth subcarbonate and desalted soft water; introducing low-pressure saturated steam (B) into a steam heating coil pipe at the periphery of an impregnating solution preparation tank through a steam inlet (1 d) of the impregnating solution preparation tank, performing non-contact heat exchange with materials in the tank, heating the materials in the tank to a certain temperature, and delivering steam condensate (C) generated after heat exchange through a steam condensate outlet (1 e) of the impregnating solution preparation tank; simultaneously starting a centrifugal pump (1-1) and a stirrer (1-2) of the impregnating solution preparation tank to enable materials in the tank to flow, uniformly mixing, fully reacting acetic acid with zinc oxide to generate zinc acetate aqueous solution, and obtaining the impregnating solution after the reaction is completed;
wherein: the temperature of the materials in the impregnating solution preparing tank to be heated is 60-80 ℃;
(2) Activated carbon packing
Firstly, sucking purchased activated carbon (D) into a gas-solid separator through a vacuum pump (3) from an activated carbon inlet (4 a) of the gas-solid separator; a filter (4-1) is arranged in the gas-solid separator (4), and the gas (E) generated after the filtration is discharged into the atmosphere through a gas outlet (4 c) of the gas-solid separator; after the amount of activated carbon added from an activated carbon inlet (4 a) of the gas-solid separator reaches a certain amount, a vacuum pump (3) is closed, compressed air (Q) is introduced into the gas-solid separator from a compressed gas inlet (4 d) of the gas-solid separator, so that the gas-solid separator is positive in pressure, and the activated carbon is conveniently blanked at the bottom of the gas-solid separator under the blocking action of a filter (4-1); activated carbon filled at the bottom of the gas-solid separator is sent to the impregnation drying tower from an activated carbon inlet (6 b) of the impregnation drying tower for filling through an activated carbon outlet (4 b) of the gas-solid separator under the action of a blower (5);
repeating the above charging operation steps until the activated carbon charged from the activated carbon inlet (6 b) of the impregnation drying tower reaches the charging amount;
(3) Cyclic impregnation
The impregnating solution prepared in the step (1) is circularly fed into an impregnating drying tower (6) from an impregnating solution outlet (1 b) of an impregnating solution preparation tank through an impregnating solution inlet (6 a) of the impregnating drying tower by a feed pump (2), and the activated carbon (D) filled in the step (2) is impregnated;
in the dipping process, hot water (F) is added into the dipping drying tower through a hot water inlet (6F) of the dipping drying tower, and non-contact heat exchange is carried out between the hot water and materials in the tower, so that the stability of the dipping temperature is ensured; hot water after heat exchange is discharged from a hot water outlet (6 g) of the impregnation drying tower; simultaneously, a certain liquid level is maintained in the impregnating and drying tower all the time, so that the activated carbon is immersed, redundant impregnating solution flows out of the tower from an impregnating and drying tower overflow solution outlet (6 e), is added into a filter (9) through a filter overflow solution inlet (9 a) connected with the impregnating and drying tower overflow solution outlet (6 e), and is filtered to remove active carbon residues, and then is recycled from an impregnating solution recycling inlet (1 c) to an impregnating solution preparation tank through a filter recycling impregnating solution outlet (9 b);
meanwhile, monitoring the concentration of zinc acetate at an overflow liquid outlet (6 e) of the impregnation drying tower, and when the concentration of zinc acetate is not changed any more, the adsorption of the activated carbon to the impregnation liquid is saturated, namely, the cyclic impregnation process of the activated carbon is completed, and the catalyst is obtained;
wherein: the dipping temperature of the dipping drying tower is 80-90 ℃; when adsorption is saturated, the concentration of zinc acetate at the overflow liquid outlet (6 e) of the impregnation drying tower is 18-21%, and the adsorption quantity of the activated carbon to the zinc acetate is 31-35g zinc acetate/100 g activated carbon;
(4) Drying of the catalyst
Closing a feeding pump (2), stopping adding the impregnating liquid into the impregnating drying tower (6), and starting a recycling pump (10); delivering the impregnating solution in the impregnating drying tower from an impregnating solution recycling outlet (6 h), delivering the impregnating solution to a filter for filtering through a recycling pump (10) from a filter recycling impregnating solution inlet (9 c), and adding the filtered recycling impregnating solution into an impregnating solution preparation tank for recycling through a filter recycling impregnating solution outlet (9 b) from an impregnating solution preparation tank recycling impregnating solution inlet (1 c);
the catalyst obtained in the step (3) is naturally dripped in an impregnating and drying tower, and then the catalyst is indirectly heated under the action of hot water pipes distributed in the impregnating and drying tower after the natural dripping and drying are finished; simultaneously, hot nitrogen (G) is introduced into the impregnating and drying tower through a hot nitrogen inlet (6 j) of the impregnating and drying tower, and the catalyst is directly heated and dried;
the dried gas carries a small amount of activated carbon powder and is discharged into a bag filter through a gas inlet (11 a) of the bag filter from a gas outlet (6 d) of the impregnation drying tower, and dust is removed through the bag filter; the gas after dust removal is sent out from a bag filter gas outlet (11 b), and the obtained powder (I) is discharged from a bag filter powder outlet (11 c);
part of the gas sent out from the gas outlet (11 b) of the bag filter is pressurized by a Roots blower (12) and is added into the heater (13) from the first gas inlet (13 a) of the heater; the rest gas sent out by the bag filter gas outlet (11 b) enters a demister through a demister gas inlet (14 a) to be cooled and demisted, and after the treatment, the demister gas outlet (14 b) is pressurized by an induced draft fan (15) and then is added into a heater through a heater second gas inlet (13 b);
introducing steam (B) into the heater through a steam inlet (13 d) of the heater, and performing non-contact heat exchange with gas in the heater; the steam condensate (C) after heat exchange is discharged from a steam condensate outlet (13 e) of the heater, and the heated gas is fed out from a circulating gas outlet (13C) of the heater and then is added into the impregnating drying tower for recycling through a circulating gas inlet (6 k) of the impregnating drying tower;
after the catalyst in the impregnation drying tower is dried, adding the catalyst into the catalyst storage tank (7) through a catalyst inlet (7 a) of the catalyst storage tank, and packaging the catalyst through a vibrating screen (8) to obtain a catalyst finished product (H);
wherein: the temperature of the hot nitrogen (G) is 80-90 ℃, and the moisture content of the catalyst after drying is not higher than 0.5%.
3. The method according to claim 2, characterized in that: in the step (1), the reaction equation of acetic acid and zinc oxide is ZnO+2HAC→Zn (AC) 2 +H 2 O。
4. The method according to claim 2, characterized in that: in the step (2), the purchased activated carbon is 28-40 meshes, the iodine adsorption value is more than or equal to 1000mg/g, the strength is more than or equal to 95%, and the water content is less than or equal to 3%.
5. The method according to claim 2, characterized in that: in the step (4), the volume ratio of the gas fed into the Roots blower to the gas fed into the demister is 7:3.
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